CN202337694U - Electron-level hyper-pure ammonia extracting device and automatic online detecting device thereof - Google Patents
Electron-level hyper-pure ammonia extracting device and automatic online detecting device thereof Download PDFInfo
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- CN202337694U CN202337694U CN2011203884947U CN201120388494U CN202337694U CN 202337694 U CN202337694 U CN 202337694U CN 2011203884947 U CN2011203884947 U CN 2011203884947U CN 201120388494 U CN201120388494 U CN 201120388494U CN 202337694 U CN202337694 U CN 202337694U
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The utility model discloses an electron-level hyper-pure ammonia extracting device, comprising a liquid ammonia storage tank, a liquid ammonia pump, a gasifying device, a degreaser, a rectifying tower, a terminal purifier, a condenser and a product storage tank. The rectifying tower comprises a first rectifying tower and a second rectifying tower, so as to overcome the limitation of the traditional hyper-pure ammonia purifying process flow, simplify the hyper-pure ammonia purifying process, greatly reduce the energy consumption of the entire production process and improve production efficiency. Furthermore, the utility model further provides an electron-level hyper-pure ammonia automatic online detecting device used on the electron-level hyper-pure ammonia extracting device. The electron-level hyper-pure ammonia automatic online detecting device comprises an analysis sampling assembly and a control system and has short sampling time, so that the online product quality state can be rapidly analyzed and shown. Therefore, the entire production process of the product is controlled.
Description
Technical field
The utility model relates to special gas purifying plant and proofing unit, particularly a kind of electronic-grade ultra-pure ammonia purifying plant and automatic on-line proofing unit thereof.
Background technology
In existing ultra-pure ammonia purifying industrial device; The operational path that adopts is similar basically; The purification devices of mentioned 7N electronic-grade ultra-pure ammonia among the disclosed electronic-grade ultra-pure ammonia of patent CN200920235917.4 purifying extraction element and the patented claim CN201010140687.0 for example; Be raw material all, through the vaporizer vaporization, then through the oil eliminator oil removing with industrial liquefied ammonia; Behind the molecular sieve adsorber drying and dehydrating, directly get into rectifying tower again, the purifier degree of depth dewaters and obtains the finished product the rectifying products obtained therefrom through the terminal again.In this technological process, though can obtain high purity product, its complex technical process at last; Ammonia is through repeatedly vaporization and condensation, and process such as absorption consume electric power such as need regenerate is excessive, and this is for today of energy growing tension; Be very not energy-conservation, cause the products production cost too high; And before rectifying, dry adsorption unit is set, and bring entering rectifying tower such as new granule foreign easily into, cause the fluctuation of quality product.
And in the process of producing ultrapure special gas, the analyzing and testing of its product is a vital link.The stability of the time of response of analyzing and testing system and analysis precision, analytical data all is related to the production of whole extraordinary high-purity gas.In the production equipment of existing domestic high gas, still adopt gas-sample analysis in the past, done two big defectives like this, the one, the timely online purity of reactor product, thereby the quality of uncontrollable production product; It two is in the sampling process of gas, might pollute the high gas sample, thereby final detection result can not actual response production, causes erroneous judgement.
Summary of the invention
The utility model problem to be solved just provides a kind of electronic-grade ultra-pure ammonia purifying plant; Broken through the restriction of traditional ultra-pure ammonia process for refining flow process; Simplify the process for refining of ultra-pure ammonia, greatly reduced the energy consumption of whole production technology, and improved production efficiency.
In order to solve the problems of the technologies described above; The utility model adopts following technical scheme: a kind of electronic-grade ultra-pure ammonia purifying plant; It is characterized in that: comprise liquefied ammonia storage tank, ammonia pump, vaporizer, oil eliminator, rectifying tower, terminal purifier, condensing surface and product storage tank, said rectifying tower comprises first rectifying tower and second rectifying tower, and ammonia pump is linked in the liquefied ammonia storage tank and with liquefied ammonia and squeezes into vaporizer; Vaporizer output is connected on the oil eliminator; On oil eliminator output was connected in the first rectifying Tata, first rectifying tower was connected to the second rectifying Tata still from cat head output, and second rectifying tower is connected on the purifier of terminal from cat head output; Terminal purifier output is connected on the condensing surface, and condensing surface output is connected on the product storage tank.
Further; The cat head of said first rectifying tower is provided with first overhead condenser that is communicated with first rectifying tower; First overhead condenser output is connected to second rectifying tower, is provided with second overhead condenser that is communicated with second rectifying tower at the cat head of second rectifying tower, and second overhead condenser is exported and is connected to second rectifying tower and product storage tank; At the bottom of the tower of first rectifying tower, be provided with first tower bottom reboiler that is communicated with first rectifying tower; The output of the first tower bottom reboiler top is connected to first rectifying tower, at the bottom of the tower of second rectifying tower, is provided with second tower bottom reboiler that is communicated with second rectifying tower, and the output of the second tower bottom reboiler top is connected to second rectifying tower.
Further, the also parallelly connected output of said first tower bottom reboiler and second tower bottom reboiler is connected to the liquefied ammonia withdrawing can.
Further, said liquefied ammonia withdrawing can is connected the bottom of first tower bottom reboiler and the bottom of second tower bottom reboiler.The liquefied ammonia of residual high concentration impurities is reclaimed.
Further, said liquefied ammonia withdrawing can is also connected with the bottom of vaporizer.The liquefied ammonia of residual high concentration impurities is reclaimed.
The utility model also provides a kind of electronic-grade ultra-pure ammonia automatic on-line proofing unit that is used on the above-mentioned purifying plant in addition, and sample time is short, can react online quality product situation at the fastest time inner analysis, thus control product whole process of production.Concrete technical scheme is following: a kind of electronic-grade ultra-pure ammonia automatic on-line proofing unit; Comprise analytical sampling assembly and system; It is characterized in that: said analytical sampling assembly comprises sampling line and analyzing and testing device, and sampling line connects purifying plant and analyzing and testing device, and said system comprises automatic valve that is located on the sampling line and the unit of controlling the automatic valve switch motion; Also be connected with the purging pipeline on the analyzing and testing device, purge on the pipeline and be connected to inert gas source.
Further; Said sampling line comprises first stopple coupon on the input channel that is connected on first rectifying tower, be connected on second stopple coupon on the input channel of second rectifying tower, be connected on the 3rd stopple coupon on the output channel at the first tower bottom reboiler top, be connected on the output of second overhead condenser is connected to the 4th stopple coupon on the transport pipe of second rectifying tower, is connected on the 5th stopple coupon on the output channel at the second tower bottom reboiler top, is connected on the 6th stopple coupon on the output channel of second rectifying tower, is connected on the 7th stopple coupon on the output channel of terminal purifier and is connected on the 8th stopple coupon on the output channel of condensing surface, the first, second, third, fourth, the 5th, the 6th, the 7th and the 8th stopple coupon parallel connection connect into analysis detector; First, second, third, fourth, be provided with automatic valve respectively on the 5th, the 6th, the 7th and the 8th stopple coupon.Sampling separately, assurance analyzing and testing result's tolerance range.
Further, said inert gas source is a helium gas source.The helium light weight, cost is lower.
Further, said analyzing and testing device output is connected in the liquefied ammonia withdrawing can.Be convenient to reclaim waste gas, reduce and pollute.
Further, also be provided with automatic valve on the said purging pipeline.
After adopting technique scheme, the utlity model has following advantage: purifying plant adopts two tower rectifying, removes light constituent and heavy constituent impurity respectively, has fully guaranteed the purity of product ammonia; Save the dry adsorption unit before the rectifying, reduced energy consumption on the one hand, also avoided on the other hand bringing into rectifying tower such as new granule foreign, thereby made the whole technology can steady running, avoided quality product to produce fluctuation; The automatic on-line proofing unit carries out sampling analysis to a plurality of points in the purifying plant respectively, and analysis detecting data is convenient to each sampling spot equipment of living in is carried out parameter adjustment, and the quality product of electronic-grade ultra-pure ammonia is further enhanced.
Description of drawings
Below in conjunction with accompanying drawing the utility model is described further:
Fig. 1 is the structural representation of a kind of electronic-grade ultra-pure ammonia of the utility model purifying plant;
Fig. 2 is arranged on the structural representation on the purifying plant for a kind of electronic-grade ultra-pure ammonia of the utility model automatic on-line proofing unit.
Embodiment
As shown in Figure 1; A kind of electronic-grade ultra-pure ammonia purifying plant comprises liquefied ammonia storage tank 1, ammonia pump 2, vaporizer 3, oil eliminator 4, rectifying tower 5, terminal purifier 6, condensing surface 7 and product storage tank 8, and ammonia pump is linked in the liquefied ammonia storage tank and with liquefied ammonia and squeezes into vaporizer; Vaporizer output is connected on the oil eliminator; On oil eliminator output was connected in the first rectifying Tata, first rectifying tower was connected to the second rectifying Tata still from cat head output, and second rectifying tower is connected on the purifier of terminal from cat head output; Terminal purifier output is connected on the condensing surface, and condensing surface output is connected on the product storage tank.In the present embodiment; Said rectifying tower comprises first rectifying tower 51 and second rectifying tower 52; Oil eliminator output is connected to first rectifying tower, and the output of first rectifying tower is connected to second rectifying tower, and the output of second rectifying tower is connected to the terminal purifier; Cat head at first rectifying tower is provided with first overhead condenser 511 that is communicated with first rectifying tower; First overhead condenser output is connected to second rectifying tower, is provided with second overhead condenser, 521, the second overhead condensers that are communicated with second rectifying tower at the cat head of second rectifying tower and exports and be connected to second rectifying tower; At the bottom of the tower of first rectifying tower, be provided with first tower bottom reboiler 512 that is communicated with first rectifying tower; The output of first tower bottom reboiler is connected to first rectifying tower, at the bottom of the tower of second rectifying tower, is provided with second tower bottom reboiler, 522, the second tower bottom reboilers output that is communicated with second rectifying tower and is connected to second rectifying tower.
In addition, first tower bottom reboiler and second tower bottom reboiler also parallel connection output are connected to liquefied ammonia withdrawing can 9, and in the present embodiment, the liquefied ammonia withdrawing can is connected the bottom of first tower bottom reboiler and the bottom of second tower bottom reboiler; Simultaneously, the liquefied ammonia withdrawing can is also connected with the bottom of vaporizer.In the utility model; Getter in the purifier of terminal is according to metal or intermetallic compound and multiple gases effects such as hydrogen, oxygen, nitrogen, carbon monoxide, carbonic acid gas, steam and methane; Generate stable compound or sosoloid; Thereby remove trace impurity, in the present embodiment, the getter that preferred zirconium ferro-vanadium is processed.
The production technique of above-mentioned purifying plant is following: industrial liquefied ammonia is stored in the liquefied ammonia storage tank, squeezes into vaporizer through ammonia pump, and liquefied ammonia is through overflash; Then through the oil eliminator oil removing; Directly get into rectifying tower and carry out the separation of weight component, the effect of first rectifying tower is a light constituent impurity of removing incoagulability at cat head, and the product of tower still gets into second rectifying tower and removes heavy constituent impurity; Metallic impurity, moisture content, wet goods organic impurities like trace; Through detecting qualified promptly filling into bottle, if each impurity composition exceeds standard, then the liquefied ammonia product gets into next operation from the product of the second rectifying tower overhead condensation; Again vaporize and get into the terminal purifier and carry out micro-removal of impurities, thereby guarantee that whole technology obtains the ultra-pure ammonia entering product storage tank of specification product quality.The liquefied ammonia of the residual high concentration impurities of vaporizer and rectifying tower reboiler bottom is recycled in the liquefied ammonia withdrawing can in the whole process.
As shown in Figure 2 in addition; The utility model also provides a kind of electronic-grade ultra-pure ammonia automatic on-line proofing unit that is used on the above-mentioned purifying plant; Comprise analytical sampling assembly and system; Said analytical sampling assembly comprises sampling line and analyzing and testing device 101, and sampling line connects purifying plant and analyzing and testing device, and said system comprises automatic valve 102 that is located on the sampling line and the unit 103 of controlling the automatic valve switch motion; Also be connected with on the analyzing and testing device and purge pipeline 104, purge on the pipeline and be connected to inert gas source 105.
In the present embodiment; Said sampling line comprises first stopple coupon 111 on the input channel that is connected on first rectifying tower, be connected on second stopple coupon 112 on the input channel of second rectifying tower, be connected on the 3rd stopple coupon 113 on the output channel at the first tower bottom reboiler top, be connected on the output of second overhead condenser is connected to the 4th stopple coupon 114 on the transport pipe of second rectifying tower, is connected on the 5th stopple coupon 115 on the output channel at the second tower bottom reboiler top, is connected on the 6th stopple coupon 116 on the output channel of second rectifying tower, is connected on the 7th stopple coupon 117 on the output channel of terminal purifier and is connected on the 8th stopple coupon 118 on the output channel of condensing surface; First, second, third, fourth, the 5th, the 6th, the 7th and the 8th stopple coupon parallel connection connect into analysis detector wherein is provided with automatic valve on the first, second, third, fourth, the 5th, the 6th, the 7th and the 8th stopple coupon respectively.
In the foregoing description, automatic valve is preferably electromagnetic valve or operated pneumatic valve, and on the purging pipeline, also is provided with automatic valve; The analyzing and testing device adopts the DID detector that the light constituent impurity in the ultra-pure ammonia is analyzed; Unit adopts dispersing control system (DCS) unit, carries out decentralised control to reaching the automatic valve that purges on the pipeline on 8 stopple coupons; Said inert gas source is preferably helium gas source, also can adopt rare gas elementes such as argon gas.The output of analyzing and testing device is connected in the liquefied ammonia withdrawing can 9 in addition.
Automatic on-line proofing unit in the utility model adds up to 8 sampling spots, wherein is respectively component composition at the bottom of the tower of cat head component composition, first rectifying tower of feed component composition, first rectifying tower of sampling and testing first rectifying tower, the feed component composition of terminal purifier, the discharging component composition and the product tank battery of terminal purifier and divides composition.The charging quality of first rectifying tower in the production process and second rectifying tower, the quality product of cat head tower still are analyzed; In addition the quality product of the import and export of terminal purifier is analyzed, and the output channel of condensing surface is promptly filled pipeline analysis.The analysis detecting data of rectifying tower can be used for the adjustment of rectifying tower operating parameters, the quality product in the stably manufactured process; The analysis detecting data of the import and export product of terminal purifier can be used for the adjustment of the parameter of terminal purifier, can be used for whether reaching the criterion of the standard of filling filling the pipeline analysis detecting data, thus with relevant valve interlocking switch, control whole production.Gather the feed component composition of first rectifying tower such as needs, through the automatic valve on DCS controlled opening first stopple coupon, sample introduction to analyzing and testing device.After sampling finished, DCS provided the automatic valve on signal at stop first stopple coupon, provided unblanking then and purged pipeline, and pipeline is purged, and when the detection signal inclusion-free, can provide signal at stop and purge pipeline valve, stopped to purge.
Claims (10)
1. electronic-grade ultra-pure ammonia purifying plant; It is characterized in that: comprise liquefied ammonia storage tank (1), ammonia pump (2), vaporizer (3), oil eliminator (4), rectifying tower (5), terminal purifier (6), condensing surface (7) and product storage tank (8); Said rectifying tower comprises first rectifying tower (51) and second rectifying tower (52); Ammonia pump is linked in the liquefied ammonia storage tank and with liquefied ammonia and squeezes into vaporizer, and vaporizer output is connected on the oil eliminator, on oil eliminator output is connected in the first rectifying Tata; First rectifying tower is connected to the second rectifying Tata still from cat head output; Second rectifying tower is connected on the purifier of terminal from cat head output, and purifier output in terminal is connected on the condensing surface, and condensing surface output is connected on the product storage tank.
2. a kind of electronic-grade ultra-pure ammonia purifying plant according to claim 1; It is characterized in that: the cat head of said first rectifying tower is provided with first overhead condenser (511) that is communicated with first rectifying tower; The output of first overhead condenser is connected to second rectifying tower; Cat head at second rectifying tower is provided with second overhead condenser (521) that is communicated with second rectifying tower; The output of second overhead condenser is connected to second rectifying tower and product storage tank, at the bottom of the tower of first rectifying tower, is provided with first tower bottom reboiler (512) that is communicated with first rectifying tower, and the output of first tower bottom reboiler is connected to first rectifying tower; At the bottom of the tower of second rectifying tower, be provided with second tower bottom reboiler (522) that is communicated with second rectifying tower, the output of second tower bottom reboiler is connected to second rectifying tower.
3. a kind of electronic-grade ultra-pure ammonia purifying plant according to claim 2 is characterized in that: said first tower bottom reboiler and second tower bottom reboiler also parallel connection output are connected to liquefied ammonia withdrawing can (9).
4. a kind of electronic-grade ultra-pure ammonia purifying plant according to claim 3 is characterized in that: said liquefied ammonia withdrawing can is connected the bottom of first tower bottom reboiler and the bottom of second tower bottom reboiler.
5. according to claim 3 or 4 described a kind of electronic-grade ultra-pure ammonia purifying plants, it is characterized in that: said liquefied ammonia withdrawing can is also connected with the bottom of vaporizer.
6. automatic on-line proofing unit that is used on the described electronic-grade ultra-pure ammonia of claim 1 purifying plant; Comprise analytical sampling assembly and system; It is characterized in that: said analytical sampling assembly comprises sampling line and analyzing and testing device (101); Sampling line connects purifying plant and analyzing and testing device, and said system comprises automatic valve (102) that is located on the sampling line and the unit (103) of controlling the automatic valve switch motion, also is connected with on the analyzing and testing device and purges pipeline (104); Purge on the pipeline and be connected to inert gas source (105), purge on the pipeline and also be provided with automatic valve.
7. a kind of electronic-grade ultra-pure ammonia automatic on-line proofing unit according to claim 6; It is characterized in that: said sampling line comprises first stopple coupon (111) on the input channel that is connected on first rectifying tower, be connected on second stopple coupon (112) on the input channel of second rectifying tower, be connected on the 3rd stopple coupon (113) on the output channel at the first tower bottom reboiler top, be connected on the output of second overhead condenser is connected to the 4th stopple coupon (114) on the transport pipe of second rectifying tower, is connected on the 5th stopple coupon (115) on the output channel at the second tower bottom reboiler top, is connected on the 6th stopple coupon (116) on the output channel of second rectifying tower, is connected on the 8th stopple coupon (118) on the 7th stopple coupon (117) and the output channel that is connected on condensing surface on the output channel of terminal purifier, the parallelly connected connect into analysis detector of the first, second, third, fourth, the 5th, the 6th, the 7th and the 8th stopple coupon; First, second, third, fourth, be provided with automatic valve respectively on the 5th, the 6th, the 7th and the 8th stopple coupon.
8. a kind of electronic-grade ultra-pure ammonia automatic on-line proofing unit according to claim 6, it is characterized in that: said inert gas source is a helium gas source.
9. according to claim 6 or 7 described a kind of electronic-grade ultra-pure ammonia automatic on-line proofing units, it is characterized in that: said analyzing and testing device output is connected in the liquefied ammonia withdrawing can (9).
10. a kind of electronic-grade ultra-pure ammonia automatic on-line proofing unit according to claim 6 is characterized in that: also be provided with automatic valve on the said purging pipeline.
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| CN2011203884947U CN202337694U (en) | 2011-10-13 | 2011-10-13 | Electron-level hyper-pure ammonia extracting device and automatic online detecting device thereof |
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| CN2011203884947U CN202337694U (en) | 2011-10-13 | 2011-10-13 | Electron-level hyper-pure ammonia extracting device and automatic online detecting device thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320623A (en) * | 2011-10-13 | 2012-01-18 | 周平 | Purification device and purification method for electronic grade ultra-pure ammonia |
| CN102502699A (en) * | 2011-10-13 | 2012-06-20 | 周平 | Purification device for electronic grade ultra-pure ammonia and electronic grade ultra-pure ammonia automatic online detection device |
| CN104155417A (en) * | 2014-08-22 | 2014-11-19 | 中国计量科学研究院 | Pre-processing system and pre-processing method of trace moisture analysis in ultrahigh-purity gas |
| CN105116102A (en) * | 2015-06-17 | 2015-12-02 | 安徽淮化股份有限公司 | Multifunctional on-line analysis and recovery apparatus for urea ammonium nitrate solution |
-
2011
- 2011-10-13 CN CN2011203884947U patent/CN202337694U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320623A (en) * | 2011-10-13 | 2012-01-18 | 周平 | Purification device and purification method for electronic grade ultra-pure ammonia |
| CN102502699A (en) * | 2011-10-13 | 2012-06-20 | 周平 | Purification device for electronic grade ultra-pure ammonia and electronic grade ultra-pure ammonia automatic online detection device |
| CN102502699B (en) * | 2011-10-13 | 2013-09-04 | 周平 | Automatic online detection device for purification device for electronic grade ultra-pure ammonia |
| CN104155417A (en) * | 2014-08-22 | 2014-11-19 | 中国计量科学研究院 | Pre-processing system and pre-processing method of trace moisture analysis in ultrahigh-purity gas |
| CN104155417B (en) * | 2014-08-22 | 2015-12-30 | 中国计量科学研究院 | The preprocessing system of trace water analysis and method in a kind of ultra-pure gases |
| CN105116102A (en) * | 2015-06-17 | 2015-12-02 | 安徽淮化股份有限公司 | Multifunctional on-line analysis and recovery apparatus for urea ammonium nitrate solution |
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Effective date of registration: 20160317 Address after: 314400, No. 38, Lu an road, Jianshan New District, Jiaxing, Zhejiang, Haining Patentee after: HAINING INDUSAIR ELECTRONICS CO., LTD. Address before: Jiaxing City, Zhejiang Province, Haining City, 314400 yuan spent on the Bridge Industrial Park Company Patentee before: Zhou Ping |
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Address after: 314400 No.38 Anjiang Road, Jianshan New District, Haining City, Jiaxing City, Zhejiang Province Patentee after: Zhejiang yingdesai semiconductor materials Co.,Ltd. Address before: 314400 No.38 Anjiang Road, Jianshan New District, Haining City, Jiaxing City, Zhejiang Province Patentee before: HAINING INDUSAIR ELECTRONICS Co.,Ltd. |
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Granted publication date: 20120718 |